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基于铜(II)配合物形成的 HPLC-紫外检测法同时测定二醇和三醇等醇类

Simultaneous determination of alcohols including diols and triols by HPLC with ultraviolet detection based on the formation of a copper(II) complex.

机构信息

School of Science, Tokai University, Hiratsuka, Kanagawa, Japan.

Graduate School of Science and Engineering, University of Toyama, Toyama, Toyama, Japan.

出版信息

J Sep Sci. 2017 Nov;40(21):4168-4175. doi: 10.1002/jssc.201700635. Epub 2017 Sep 26.

DOI:10.1002/jssc.201700635
PMID:28851084
Abstract

We developed a reversed-phase high-performance liquid chromatography method with ultraviolet detection using on-line complexation with Cu(II) ion for analysis of five alcohols including diols and triol (methanol, ethanol, 1,2-propanediol, 1,3-propanediol, and glycerol). The Cu(II) ion concentration in the mobile phase had a great influence on the peak areas of these alcohols, but not on their retention times. Column temperature (25-40°C) and pH of the mobile phase did not affect the separation of analytes. The optimum separation conditions were determined as 5 mM CuSO , 3 mM H SO , and 3 mM NaOH at 30°C. The ratio of the peak areas for three alcohols (methanol, 1,2-propanediol, and glycerol) was in good agreement with that calculated from the obtained stability constants, molar absorption coefficients for the 1:1 Cu(II) complexes with the three alcohols, and the injected molar quantities. This fact strongly suggests that the observed high-performance liquid chromatography signals resulted from formation of the 1:1 Cu(II)-alcohol complexes. Using the proposed method, these five alcohols in spirit, liquid for electronic cigarette, mouthwash, and nail enamel remover samples were successfully analyzed with only a simple pretreatment.

摘要

我们开发了一种反相高效液相色谱法,使用在线与 Cu(II)离子络合,用于分析包括二醇和三醇在内的五种醇(甲醇、乙醇、1,2-丙二醇、1,3-丙二醇和甘油)。流动相中的 Cu(II)离子浓度对这些醇的峰面积有很大影响,但对保留时间没有影响。柱温(25-40°C)和流动相的 pH 值不影响分析物的分离。最佳分离条件确定为 30°C 时 5 mM CuSO 4 、3 mM H 2 SO 4 和 3 mM NaOH。三种醇(甲醇、1,2-丙二醇和甘油)的峰面积比与从获得的稳定常数、三种醇与 Cu(II)的 1:1 络合物的摩尔吸光系数以及注入的摩尔量计算出的比相符。这一事实强烈表明,观察到的高效液相色谱信号是由 1:1 Cu(II)-醇络合物的形成引起的。使用所提出的方法,仅通过简单的预处理,就成功地对酒精、电子烟液、漱口液和指甲油去除剂样品中的这五种醇进行了分析。

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